Log in

View Full Version : Aceton Peroxide... Where???


Nope
August 24th, 2003, 02:41 PM
I've tried to make AP for 5 times and I failed.

I'm using 85% Aceton, 30% HP and 15% HCL.

Okay, when I mix the aceton and the HP it starts heating and I cool it without knowing the temprature. After that, I pour the acid in small quanities at a time and let it cool again. And then no white precipitate is forming.

Any help would be appreciated.

Thank you.

(Using Megalomania's amounts.)

Titanium
August 24th, 2003, 02:56 PM
Have you tried to let it stay in the fridge in about 12 hours???

Nope
August 24th, 2003, 02:59 PM
Yes, but not 12... 4 hours.

Rhadon
August 24th, 2003, 03:05 PM
I really didn't think that someone could be able to mess up an actone peroxide synthesis! What a pity that I don't have administrative powers in this section :).

Just in case this topic will stay here long enough for you to answer: It would be good for us to know what the other 15% of your acetone are. And: How much HCl did you use (in relation to the amount of hydrogen peroxide and acetone)?

Anthony
August 24th, 2003, 04:10 PM
Are you sure that's 30% H2O2 you have and not 30vol? Where did you get it from?

If it is, you'll have to leave it for at least 24hrs before you can expect any crystal formation.

Arthis
August 24th, 2003, 07:38 PM
Anyway, when making AP you can let it sit for 24 hours, unused acetone will be evaporated, and as AP is not soluble in water, it wil result very little losses.

The acetone can be impure due to mixes with another products, like nail remover, some spray to clean up kitchen or windows (I think there are some using aceton). And then further concentrated. There are always special products in each country; using different chemicals...

Cyclonite
August 25th, 2003, 07:43 AM
Man...Have you looked at my AP in Iraq thread? If I can here you can there. Let it sit for longer as stated and try and vary the % of chems. Experiment and see what works best for you, take a look at all the AP synth information mentioned and try those.

DBSP
August 25th, 2003, 08:15 AM
The acetone impurities may be ethyl acetate. It is availible here as a substitute for acetone in nail varnish removers so it might be a mixture of the two. I don't know wether ethyl actetate dissolves AP but if it was very effective at doing that it could perhaps lower the yileds. I strongly doubt that because of all the water though.

Nope
August 25th, 2003, 01:51 PM
No. It's 30%. I got it from a medical supplies shop. I'll try again and let it cool for 24 hours this time.

T_Pyro
August 26th, 2003, 06:15 AM
If you got the hydrogen peroxide from a medical supplies shop, it could be either 6% w/v (which is what I use), or 27% w/v (which is harder to find, but reacts faster). Acetone is generally easy to find (and cheap, too) in the pure state (100%), the medical supplies shop should have it. 0.1 N HCl / H2SO4 are just fine.
4 hrs?? You gotta be patient!! I use 6% hydrogen peroxide, 100% acetone, 100 ml 0.1 N HCl, and I have to wait for about a week and a half till any substantial amount of ap is formed. The reaction mixture is kept in a refrigerator at 3* C all the while. Try keeping it cool for about 24-48 hrs.
Another thing- when you said that the reaction mixture gets heated, do you mean in excess of 30 degrees C ? That doesn't sound too safe- you could end up with more of the dimer (much more unstable) than the trimer (relatively more stable) if the reaction is allowed to proceed at such temperatures. Why don't you cool all the reactants to about 4 degrees C in a refrigerator before making the ap? Also, remember to use an ice bath to keep the reaction temperature low, and add the acid very slowly, stirring with a glass rod all the while.
DBSP, Yup, it is highly probable that ethyl acetate dissolves AP (both are non-polar compounds, both ketones, and like dissolves like), but I doubt that it would affect the yields...

metafractal
August 26th, 2003, 07:51 AM
If ethyl acetate does dissolve AP (which seems likely as you point out), then how could it not affect yields?
The ethyl acetate dissolves the AP, and it becomes a solution. Therefore when he filters it less appears as, while the AP is there, it is not in a crystalline state.
And you are clearly exaggerating when you say a week for 6% H2O2. Once I left a batch to sit under the conditions you described for a week and it formed a solid cake at the bottom! 48hrs is plenty, and the times he described should be plenty for 30% H2O2.

Desmikes
August 26th, 2003, 12:08 PM
Nope, how much of each compound did you use? I'm having difficulty believing that you cannot find pure acetone. Unless you are sure that your H2O2 is 30% I'd try a peroxide burn test. Other than that, the only thing that might keep you from getting your AP is if you follow directions that were based on higher concentratioin of acid (usually it's around 35%), might wanna add more or try some other acid.

Nope
August 26th, 2003, 02:29 PM
The Hydrogen Peroxide is 30%. I told the man who has the shop to make 30% H.P.. Yesterday, I got aceton from a paintstore but there wasn't any concetration noted in the container's label. I use 200ml. H2O2, 150ml. Aceton and 50ml. HCL (15%). Next time, I'll let it cool in the freezer for 1-2 days.

kingspaz
August 26th, 2003, 06:23 PM
you told him to make 30% H2O2? haha
you know it sounds like? the guy in the shop is a fucking retarded ape. i suspect hes made a 30% solution using 6% peroxide or something similar. that is, 30% of 6% peroxide solution. thus, a 1.8% peroxide solution. assuming he started with 6%.

Nope
August 26th, 2003, 06:38 PM
I know that guy and he gave me 30% of 100%. Κακομοίρη μαλακα. :)

knowledgehungry
August 26th, 2003, 06:39 PM
No one has 100% H2O2, it is EXTREMELY unstable.

Nihilist
August 26th, 2003, 06:45 PM
could use good 'ol fashioned sunlight. H2O2 decomposes in the presence of ultraviolet rays, though i'm not sure how quickly.

Rhadon
August 26th, 2003, 06:56 PM
Nihilist is referring to a post of myself which I deleted because Nope already stated that he's sure that his H2O2 is 30% before I was able to submit my post. I suggested to test the H2O2 content by decomposing it with a catalyst and looking if many bubbles form.

I don't think that the decomposition of H2O2 under sunlight is fast enough for measurement with the eye, though. MnO2 or silver should be better. Using HCl and measuring the Cl2 created should be better.

T_Pyro
August 26th, 2003, 10:31 PM
Why not do the test in a closed environment, and collect the o2 formed in a graduated cylinder using downward displacement of water, and after measuring the volume of o2 formed, calculate the purity of the H2O2?

metafractal, the amount of ethyl acetate impurities that might be present will not be able to dissolve significant quantities of ap, hence it should not make much of a difference. Oh, and I was not exaggerating when I said a week. If I keep it for a day or two, I only end up with about 1.5 Gms of ap... not worth it. Leaving the reaction mixt. outside makes it worse, because in that case, I just get bubbles of o2, no ap. 30% h2o2 is worlds apart, though, and I guess 12-24 hrs would do, like you said... What was the temperature and light conditions when you did your expt. for a week?

vulture
August 27th, 2003, 03:51 AM
I suspect the whole problem of this thread lies in the fact that some people are just too retarded to get the difference between volume%/weight% and mass/volume/density.

Rhadon
August 27th, 2003, 04:59 AM
Why not do the test in a closed environment, and collect the o2 formed in a graduated cylinder using downward displacement of water, and after measuring the volume of o2 formed, calculate the purity of the H2O2? Because I'm afraid all this would get too complicated for Nope, so I chose the easiest method I could imagine. It will be good enough for distinguishing between 1.8% and 30% H2O2.

metafractal
August 27th, 2003, 05:45 AM
T_Pyro: I see your point. When I left the AP for a week it was at about 7*C (I usually keep it at more like 3*C, though) and it was exposed to sunlight/moonlight throgh plastic(the reaction vessle was kept outside with artificial temperature control). It might have had something to do wit hthe fact that I used a jam jar and not pyrex glass...
But seriously, those yields are worrying. What protocol do you use? Take a look at angelo's (http://www.geocities.com/angelo_444/3to6.html). This is the one I use for 6%. While I have never achieved the yields he shows, I have found it to be the best method for low conc. H2O2. Its not too bad for high conc. H2O2 either, if the amounts are adjusted appropriately.

kingspaz
August 27th, 2003, 02:47 PM
knowledgehungry, that was my thinking too. even IF he had 100% H2O2 theres no way in hell he'd handle it. unless he IS retarded as i suspenct is the case.

nope, did the guy you buy it off have a fat neck?

Desmikes
August 27th, 2003, 10:10 PM
or instead of a catalyst you could just get your skin wet w/H2O2 and see if it turns white (it will go away in a few hrs) that's what I met by peroxide burn. If it does it very quickly then you prbly do have 30+ conc. this thread really is going nowhere though

Cyclonite
August 31st, 2003, 03:57 AM
Ok, iv heard people say that when they put in the acid that AP started to from immediately filled the container in a short amount of time while other wait 1 week? I know the concentration of chems has alot to do with it but does it really form that fast with high concentration chems?

metafractal
August 31st, 2003, 04:42 AM
No, it does not :).
I have made AP with everything from 3% to 50% H2O2. While concentration does make a huge difference, both of the extremes you mentioned are unrealistic. Those who wait a week are either using a riddiculously low concentration H2O2 (<2%) or are doing something terribly wrong. The only conditions under which AP can form that quickly are undesireable. If, say, you use high conc H2O2 with excess H2SO4 catalyst and no heat control (i.e. no ice bath) then yes, your AP will form very quickly. However, you will end up with a poor yield of almost totally dimer, give off some nasty fumes, and generate enough heat for there to be a risk of detonating the formed AP!
So, to answer your question, under healthy conditions AP should take between ~1.5 hrs (>30% H2O2) and ~72 hrs (3% H2O2) to form. Yes, concentrations do make a big difference, but not as big as you said. If it takes much longer or much shorter you are doing somethign wrong.

DBSP
August 31st, 2003, 09:09 AM
When I use 35% H2O2 5h is about enaugh. I've reacted it longer without getting any increased yields.

But one time when I made some AP with 19.5% H2O2 something must have gotten really fucked up because after 2 days there was only as small ammount of AP formed. After a weak the yield was the expected but thats about at least 4 days longer than normal. Same retios was used as always, same cooling too.

Thing is you never know about chemestry, sometimes things get fucked up, it's just the way it is..

T_Pyro
August 31st, 2003, 12:21 PM
metafractal, what volume, and what normality (basically, how many equivalents) of sulfuric acid do you use? I am not using "a riddiculously low concentration H2O2 (<2%)". What I use is 6% w/V (That's 6gm H2o2 per 100 ml of H2O). If anything's wrong, it can only be the acid. I'm using 0.1 N , 100ml HCl (That makes it 0.01 equivalents). What concentration do you suppose I should be using? I use 100 ml acetone (100%) , 400 ml H2O2 (6%)

DBSP
August 31st, 2003, 02:37 PM
Well first of all you are using too little acetone, 150ml is more apropriate. 400x0,06=24, 24x06=144ml.

I always use 30% HCl as catalyst, 10% of total ammount of reactants(acetone+H2O2).
But you should probably be using more because of your low conc H2O2.

THErAPIST
September 1st, 2003, 03:11 AM
100 ml 25% h202
70ml 100% acetone
50ml 32% HCL

I react my mixture in a bowl of cold water with a few ice cubes. I let it sit in the ice bath until all the acid has been stirred in and then I let it sits in the ice bath for another 5 minutes. It is then taken out and left at whatever temperature it is outside at the time for another 50 minutes or so. My reaction is done is an hour. The bottle is usually full of a pretty dense mess of AP which has been stored for periods of 6 weeks dry just to see what would happen. It seemed to be just as powerful, just as stable as the stuff that was made in the freezer (which took 3 days), the reaction was faster, and I got a better yield when it wasn't in the freezer.

Before anyone decides to tell me how stupid I was to store it dry; it was set in a plastic jar with a rubber lid that did not screw on or snap on in the woods in the spring... I also opened it up with a tent pole just incase it went off. After a good bit of poking and prodding I found it to be just as stable as it was when I put it there.
I'm mainly saying this just so that people dont think that AP can't be made quickly with high yield and desireable properties. I guess it just depends on the experimenters preferences.

Am I the only one who can say I've tested the difference between trimer and dimer?

And to Nope... Many people have trouble with Mega's AP synth but they have no trouble at all with other peoples synths. Experiment. DO NOT use my synth though as you'd likely kill yourself. I sat there watching my AP reaction the whole time to make sure it didnt runaway, and most people would call me extremely insane/ mongloidish for purposly making AP at an elevated temp.

ALENGOSVIG1
September 1st, 2003, 06:21 AM
Awhile ago i did an experement making AP at elevated temperatures. I heated 35 ml of H2O2/acetone until it was almost boiling, and added 5 ml of 28% HCl. Within less than 30 seconds some AP formed and the solution became cloudy with precipitate. Within a couple minutes the solution was boiling, and emitting some very nasty fumes which had an unpleasant tear gas effect to say the least. The AP which had formed was no longer visible, as it must have dissolved/sublimated. I placed a tupperware container over the beaker and within a few minutes there was a thin layer of recrystallized AP coating the inside of the tupperware container.

When the reaction subsided. There were small droplets of oil (molten AP:D) on the surface. After the solution returned to room temperature, a cake of solid AP was floating on the surface of the liquid.

THErAPIST
September 1st, 2003, 06:43 AM
EEEEEWWW! See that's happened to me once but when it happened to me I was using 50% H2O2 and the beaker slipped out of my hand pouring it all in at once (I was adding the H2O2 to the acid/ acetone instead of acid to the H2O2/acetone) It almost immedietly started spewing some sort of clearish gas with an ungodly amount of heat. I was in a bad place with it so I attempted to move to a better place and got a face full of that gas. I couldnt open my eyes for a good 2 hours without them burning so badly that I wanted to close them again. Sad thing was every time I closed em they started to hurt more. Possibly the worst night I had had in years :(

I didn't get a solid cake of AP then though. I got an oil that was on the bottom of the rest of the liquid that was still in the flask (which wasn't flammable)

I know we're starting to stray off topic a bit , (it might help the new guy though?) but did you do any testing with your dimer compared to trimer? Stability? Performance?

T_Pyro
September 1st, 2003, 08:36 AM
Thanks guys, next time, I'll jus use more of acetone & more acid. :) DBSP, correct me if I'm wrong, but don't the acetone and the peroxide react in equimolar ratios? That's what I gathered while looking through the reactions stated on Megalomania's page on AP. I calculated the amount of acetone that I would require for 400ml 6% H2O2, and it turned out to be about 76ml, so I use 100 ml since that's the amount in the bottle anyway, and I thought an excess of reactants would enable the reaction to proceed to completion.

ALENGOSVIG1, when you said "elevated temperatures", what would be the actual temperature? 90*C? I've never made AP at such high temperatures- any idea what the melting point of AP is? Also, in what form does it exist in the liquid state? Does it still exist as a dimer/trimer, or does the chain get broken? THErAPIST, the "oil" that you found at the bottom of the reaction vessel, what exactly was it? Pure AP? Some sort of AP solution in acetone? Did it crystalize out? If so, what was its stability like? Sorry for all the questions, but this is the first time I'm hearing of liquid AP:confused:

THErAPIST
September 1st, 2003, 02:01 PM
I'm not completely sure what that oil was that I got. I tried a flame test and it didn't catch on fire so I collected it in a film can and put a blasting cap in there... didn't do a damn thing besides break the film can. I simply had a runaway reaction. I've been told that the oil which was produced was most likely oxidised acetone but I thought that acetone couldnt be oxidised anymore :confused:

I'm not positive as to how hot ALEN's reaction was but I'm guessing in the range of 70 to 80ΊC. Ive also read that the melting point of AP is a whole 20 degrees or so below the decomposition temp. Leave it to the retarded arse terrorist/ suicide bomber fags to try and cast AP:rolleyes:
The AP at an elevated temp would be dimer though. As far as I know AP cannot exist in a liquid state unless you're trying to cast it/ kill yourself.

Mumble
September 1st, 2003, 02:49 PM
AP melts a little below 100 degrees. I believe it is something along the lines of 90 to 95. Megalomania has it listed at 91. I don't really plan on finding the exact value personally.

I wouldn't imagine the Acetone/H<sub>2</sub>O<sub>2</sub> mix would go much above 70 without boiling. Pure acetone boils at 56 degrees. I'm not exactly sure how much the boiling points are changed by each other, but 70 seems pretty reasonable to me.

T_Pyro
September 3rd, 2003, 12:18 AM
THErAPIST- Could the oil have been some higher alkane? You said that the oil was most probably oxidized acetone... Mebbe the -CO- group got oxidized to CO2, leaving 2 methyl radicals, which could combine to form a higher alkane?

THErAPIST
September 3rd, 2003, 03:03 AM
My chemistry book doesnt say much about alkanes, But from what I just read it seems to be quite possible some of the acetone could have been converted to a higher alkane. According to my book there has to be pretty high temperatures for alkanes to change. In this case the reaction wouldnt have to be all THAT high i dont think since acetone has a boiling point of a whole 57Ί, and the reaction that made the oil was most certainly a very exothermic reaction.

User Name
September 8th, 2003, 12:25 AM
While most everyone else is off topic... I have a question that concerns HE's but i didnt want to start a new thread in the HE's section because im a "newb", and yes i have searched the forum from A-Z and found nothing helpful for my embarasing situation.

My question is this, I have made APAN using my tried and true method of making AP and then simply adding finley powder furtilizer grade Ammonium nitrate. There is no wax or additives in the AN. the APAN ratio is 1:1

I have tried several times to detonate APAN but everytime i get the same results, a high pitched AP detonation sound but no thud or smoke from AN detonation. There is also AN left at the site. I have used as much as 400 grams in one charge. my charges are electronicaly detonated with 10g AP dets and burried underground a few inches in a 2inch by 2 inch PVC pipe with end caps.
my dets work very well so its not that.

Any opinions on what the problem might be would be grately appretiated.

THErAPIST
September 8th, 2003, 01:50 AM
All I can say is that your AN needs to be extremely finely powdered and extremely dry. The optimum AN to AP ratio if im not mistaken is 12% AP to 88% AN by weight. Are you pressing your APAN into the tubes or are you just simply letting it set loosly inside the pvc with the det sitting ontop of the mix?

User Name
September 8th, 2003, 10:49 AM
I have tried them pressed and unpressed with the det in the very center. and yes the optimum ratio is 12:88 AP/AN but 1:1 i thought would have a better chance of detonating the AN

I have a huge (1 gallon) batch of Acetone/H202/hydrochloric acid in my freezer. This amount normaly gives me about 5 film canisters full of completely dried AP. But this time, there is a small layer of liquid on the top of the batch. it isnt as cloudy as the rest, almost looks like water....any ideas on what it might be?

thx

Cyclonite
September 8th, 2003, 10:54 AM
Well you said you added it, im sure you mixed it but did you mix it well? Use AN right out of the oven well wait for it to cool at least. If the confinement is stronger than there will be better chance of a full detonation, keep in mind what you use for a container also is the fragmentation that is going to fly at you.

User Name
September 8th, 2003, 10:57 AM
My PVC container for confinment is underground, and my AN is very well mixed but i didnt dry it in the oven. i live in Arizona and it was 108 degrees out yesterdy. thats an average temp with no humidty so i just simply lay the AN on some aluminum foil out in the sun. seems as dry as can be when i add it.

well ill keep testing thx again guys.
oh and just soemthing ive noticed...AP wont synthesize if you get the mixture too cold (around -10c i think) it doesnt freeze it just stops making AP.

T_Pyro
September 8th, 2003, 11:56 AM
Quote: "AP wont synthesize if you get the mixture too cold (around -10c i think) it doesnt freeze it just stops making AP."

Whenever I let my ice bath get too cold (less than 0*C) then the reaction mixture does starts freezing, and when it is thawed after that, the yeilds are dramatically reduced. That is probably due to the destruction of the peroxy linkage in H2O2 once the ice crystals start forming. Are you sure you have the temperature right?

Cyclonite
September 8th, 2003, 12:45 PM
Out of the 2 forms of AP, is there really a difference to the point of it being noticeably more hazardous or powerful? The synth takes so much less time and gives a better yield with a moderate temp.

Anthony
September 8th, 2003, 03:35 PM
I appreciate the heat of the Arizona climate, but I think it still isn't enough.

AN really needs at least an hour spread out in an oven set to at least 100*C. Obviously you can't subject AP to this treatment.

I don't see any advantage to mixing the AN into the AP solution. You can get it intimately mixed enough by simply diaper mixing the dry components. Considering what a royal pain AN is to dry, I'd never get it needlessly wet.

In short, I think that mixing your AN into your AP solution is stopping you from having your AN sufficiently dry to detonate.

User Name
September 8th, 2003, 09:37 PM
ok thanks for your help. and yes im sure my temp is right. it wont start forming ice untiil it gets well below 0c and i have not noticed a difference in "power" or sensitivity in AP. ive made it without cooling at all and it seems the same (yes i tested it) as long as you wash it...its the same (from what ive noticed)
has anyone ever had washed AP sudenly detonate for no reason?

where might i get 30% H2O2??? i cant find it anywhere!
The batch i have in the freezer right now did soemthing strange...i took it out to stir it (i always stir it after 12 hours) and then i put it back in, well the AP disapered! im pist cause my huge (one gallon) batches cost 10$ each.

wha'ts the bigest AP charge any of you have detonated? ive done 200g at a time, i was only 25 feet away behind a huge boulder with eye and ear pertection. WOW

DBSP
September 9th, 2003, 10:06 AM
Please put your location in your profile it makes it easier to help you. I assume your from the states so try hydrophonic or pool acessory stores, thay normally carry 27% H2O2 as baquacil. Had you searched you would have easily found that on your own, so in the future search before posting questions that is deemed to have been discussed in the past, most things have been discussed by now.

The 12% AP to 88% AN ratio is the OBd APAN ration, however there is nothing that says it's the optimum ratio for APAN. What the optimal ratio is depends on what the APAN is to be used for, demolition, eart moving, cheap axplosive to play with etc. The less AP the cheaper and less brisant, the more AP the more expensive and brisant it gets. So it's a question of what it is to be used for.

This thread has really gone wild, the last part of it should in my oppinion be moved to the APAN topic as it more or less is what has been discussed the last posts.

And I have no idea to why your AP dissolved when you stirred the mixture.

I had a though the other day, perhaps a new AP topic could be started in the WC where people could discuss whatever they like concerning AP since more or less all AP topics soon change to APAN or where to get H2O2 topics.

User Name
September 9th, 2003, 11:32 AM
sorry about changing the subject a little but everyone else did and i couldnt find any other threads on APAN.
I live in arizona, USA. ill put that in my profile.
i have called around for H2O2 but with no prevail.
i just checked the AP batch that desolved and its still gone. i had about 5 film canisters of ap in the bottom of the jar, then i stir it and it disaperes! :) lol

DBSP
September 9th, 2003, 12:44 PM
So you couldn't find -->THIS<-- (http://www.roguesci.org/theforum/showthread.php?s=&threadid=115) thread then :confused: A 528 reply APAN topic.

A SEARCH (http://www.roguesci.org/theforum/search.php?s=) for 'APAN' yielded 97 hits.

As I said most things have been discussed and will be found with a simple search, maby just not right away.

If you haven't read the rules read them or reread them, read the sticky thread in the water cooler if you haven't read that one yet as well.

T_Pyro
September 9th, 2003, 04:13 PM
"The batch i have in the freezer right now did soemthing strange...i took it out to stir it (i always stir it after 12 hours) and then i put it back in, well the AP disapered! "

That happened to me once, but the reason for that was that I had left the mixture in the freezer for too long, so it froze up, the AP crystals got destroyed, and when I thawed it, all I was left with was a turbid mixture (which turned transparent after a few hours), and a lot of bubbles.

When your AP "disappeared", did you notice anything unusual about the reaction mixture? eg. Formation of bubbles/ the mixture turning colourless etc. If you had bubbles forming, then most probably your H2O2 just decomposed to give O2 and H20 - that happens at elevated temperatures, or even in the presence of a catalyst. What did you stir the mixture with? It is possible that it could catalysed /initiated the decomposition of the peroxy linkage.

User Name
September 9th, 2003, 10:58 PM
yes there was still alittle AP and it had bubbles in it.

yes i have read the rules and im sorry. i didnt do a search i only looked at the threads from the last 30 days.

it wont happend again.